Sodium hydride → 1-(4-Chloro-6-methyl-2-pyridinyl)ethanone O-[(2,6-Dimethoxyphenyl)methyl] Oxime

HRID 1357033

반응식

HRID 1357033 반응식
[Cl:1][C:2]1[CH:7]=[C:6]([CH3:8])[N:5]=[C:4]([C:9](=[N:11][OH:12])[CH3:10])[CH:3]=1.[H-].[Na+].[CH3:15][O:16][C:17]1[CH:24]=[CH:23][CH:22]=[C:21]([O:25][CH3:26])[C:18]=1[CH2:19]Cl>CN(C)C=O>[CH3:26][O:25][C:21]1[CH:22]=[CH:23][CH:24]=[C:17]([O:16][CH3:15])[C:18]=1[CH2:19][O:12][N:11]=[C:9]([C:4]1[CH:3]=[C:2]([Cl:1])[CH:7]=[C:6]([CH3:8])[N:5]=1)[CH3:10]

참가 물질

5

반응물 3

HCID 24758Sodium hydrideHCID 127070022-(chloromethyl)-1,3-dimethoxyBenzeneHCID 1363883511-(4-Chloro-6-methyl-2-pyridinyl)ethanone oxime

생성물 1

HCID 731784321-(4-Chloro-6-methyl-2-pyridinyl)ethanone O-[(2,6-Dimethoxyphenyl)methyl] Oxime

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

실험 절차

On the other hand, 1.66 g (9.0 mmol) of 1-(4-chloro-6-methyl-2-pyridinyl)ethanone oxime was dissolved in 15 ml of N,N-dimethylformamide, and the resultant solution was added with 0.18 g (4.39 mmol) of sodium hydride (60%, oiliness) while cooling the solution with ice. The mixture was stirred for 15 min. at a temperature below 0° C. and was added with the whole amount of the crude product of 2,6-dimethoxybenzyl chloride prepared previously while cooling the mixture with ice. The resultant mixture was stirred for 2.3 hours at a room temperature to complete a reaction. The reacted mixture was then poured into ice water. At that time, the target compound was precipitated in the ice water. The precipitation was taken out by filtering, washed with hexane and dried to thereby obtain the target compound in an amount of 2.3 g.

후처리

  1. temperaturewhile cooling the solution with ice
  2. customprepared previously
  3. temperaturewhile cooling the mixture with ice
  4. customa reaction
  5. customAt that time, the target compound was precipitated in the ice water
  6. customThe precipitation
  7. filtrationby filtering
  8. washwashed with hexane
  9. customdried
  10. customto thereby obtain the target compound in an amount of 2.3 g

출처 및 근거

ORD 기록
ord-55117f21121146beabd2e6f74c49a34b
출처 데이터셋
uspto-grants-2003_07
특허 번호
US06589967B1

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